Process of producing silicon-rayon



Patented at. 11, 1936 v 2,030,739

UNITED STATES PATENT OFFICE r I PROCESS OF PRODUCING SILICON-RAYON Rudolph S. Blcy, Elizabethton, Tenn., asslgnor to North American Rayon Corporation, New York,

N. Y., a corporation of Delaware No Drawing. Application October 22, 1934,

Serial No. 749,488

8 Claims. (01. 106-40) The present invention relates to a process of luster cellulosic products obtained therefrom, preparing cellulosic spinning solutions from have the great disadvantage of being inflammawhich soft-lustre products, such as filaments, ble, while vegetable oils become rancid and form yarns, ribbons, films, etc., may be produced. skin-irritating acids.

The primary object of my invention has to I have, unexpectedly, found that aliphatic silii wi t p a on of aliphatic silicon con compounds possess properties which render compounds into cellulosic spinning solutions, them especially suitable as delustering agents such as viscose and cuprammonium cellulose, for rayon products since they are very little inwhich will yield upon extrusion or molding softflammable and do not form irritating compounds. 1 lustre products of pleasing hand. The following table depicts a number of aliphatic Another object of my invention relates to the silicon compoundswhich may be used to deluster admixture o Silicon D V 8 h u cellulosic products, although I wish to emphasizeture R.SlHa in which R represents an alkyl radithat my invention is not limited to these comcal, with viscose and cuprammonium cellulose. pounds since others may be used with equal A third object of my invention has to do with success. I the incorporation of silicon compounds into TABLE viscose and cuprammonium cellulose solutions, saidc ompou'nds having the structure R.SiH3.OH in which R. represents an alkyl radical.

I. Derivatives having the structure 12.8111:

Boiling or A fourth object of my invention has to do with 9 melting point the dispersion of silicon compounds in the aforementioned cellulosic solutions, these com- 1mm: centi- Methylqnonosflang W 2 0 31 which R represents an alkyl radical. E 322 23; ig}

A fifth object of this invention relates to the l fiiiifignm 2mm formation of novel, soft-lustre products per se lsoflmi'i-monosilane 275-279 Al hi 11 ml laralk l-sil as. containing aliphatic silicon compounds. so 2 er 0 y an Other objects of my invention will become apparent to those skilled in the art after a study Derivatives having the structure R'SzHZ'OH of the following specification. Boning f 5 In the early days of rayon manufacture, the melting point demand was entirely for yarns having the highest possibledegree of lustre. Later, when it was Duvet-1 cm!!- found that highly lustrous rayon too clearly indimnm mm m e 154 cated its origin-an artificial fibre-Pa demand f w i 1106-2118 55 arose tor artificial silk which more closely apgg g iffiiattt" 269470 proximated to natural silk. The earliest attempt Also higher molecular alkvlsilanolsto meet the demand of dull-lustre viscose yarn, for example, was a method of retaining sulphur III. Derivatives having the structure R.Si0.0H particles in the fibres by discontinuing the norto mal desulphurizing step during its manufacture. i Compound p Although this yarn showed decreased lustre, due to scattering of light by the sulphur particles, it smwmmtic acid Sand. was impermanent and exhibited an unattractive Siliconropionic acid Do. .bloom". This method has been improved by ai -gagg 8:

dispersing, instead of sulphur, fine inorganic or Also higher-molecularsilicon-iattyacid compounds. organic particles and globules in cellulosic spinhing 501111510118, for e P ments, hydrocar- In addition, I have found that other aliphatic bons, oils, etc, When inorganic compounds, such silicon compounds may be used for the purposes, as titanium dioxide, silica, etc., are dispersed in set forth above, such as tetraethyl-monosilane, cellulosic spinning solutions, they tend to cut the triethyl-chlorethyl-monosilane, triethyl-acetoxytread guides through which the yarns are led ethyl-monosilane, halogenated monosilanes, tetduring the extrusion process, and in addition they rapropyl-monosilane, tripropyl-monosilane, triweaken cellulosic yarns considerably. Hydroisobutyl-monosilane, triiscamyl-monosilane, tetcarbons, emulsified with spinning solutions to deraisoamyl-monosilane, triethyl-ethoxy-monosilto the solution, may be varied at will.

ans, triethyl-monosilanol, siliconheptyl carbonic acid, triethyl-silicon chloride, triethyl-silicon bromide, silicon heptyloxide, .tripropyl-monosilanol acetate, tripropyl-monosilyl bromide, bis- (tripropyl-monosilyl' ether) 'triisobutyl-monosilyl bromide, triisoamyl-monosilyl bromide, bis- (triamyl-monosilyl ether), monosilyl derivatives of an city-compound, derivatives of monosilandiols having the structure R.BiH( OH) methyl-orthosilicic acid-triethylester, ethylorthosillcic acid-trimethyiester, ethyl-orthosilicic acid-triethylester, orthosllico-butyric acid-triethylester, orthosilico-isocaproic acid-triethylester, etc.

Example About 1 to 30% of an aliphatic silicon compound is dispersed in, and/or. emulsified with a cellulosic spinning solution, such as viscose and cuprammonium cellulose, the aforementioned percentage being based upon the cellulose content of the solution. After uniformly distributing the delustering agent in the spinning solution, it is extruded through suitable spinning nozzles into a conventional spinning bath. The solution may also be used for forming films or molding articles. Organic solvents, inorganic or organic pigments, etc., may be added to the spinning solutions besides silicon compounds. The amounts of aliphatic silicon compounds, added In this manner more" or less delustered rayon products may be obtained.

' Modifications of my process will readily be recognized by those skilled in the art, and, I desire to include all those modifications falling within the scope of the appended claims. In these claims, the term aliphatic silicon compound is limited to such compounds which are substantially water-insoluble and resistant to attack by alkalis and acids of such concentrations conventionally used in the rayon art.

I claim: u 1 1. A spinning solution for the manufacture of soft-lustre products comprising a solution of the group consisting of viscose and cuprammonium cellulose and a silicon compound having the structure R.SiHa, in which It represents an alkyl radical, said compound being liquid and stable in said spinning solution.

, 2. As a new article of manufacture. r senerated cellulose containing a liquid finely dispersed silicon compound having the structure RBiHa, in which R represents an alkyl radical.

3..A spinning solution for the manufacture 0! soft-lustre products comprising a solution of the group consisting of viscose and cuprammonilun cellulose together with a substance of the group consisting of aliphatic silicon compounds having the structure RBiH: in which R represents an alkyl radical, aliphatic silicon compounds having the structure R.SiH(OH)2 in which It represents an alkyl radical and aliphatic silicon compoimds' having the structure R.-.SiHz.OH in which R represents an alkyl radical, said substance being stable in said solution.

4. A spinning solution for themanufacture of soft-lustre products comprising a solution of the group consisting of viscose and cuprammonium cellulose together with a silicon compound having the structure RBKOH): in which R represents an alkyl radical, said compound being stable in said solution.

5. A spinning solution for the manufacture of soft-lustre products comprising a solution "of the group consisting of viscose and cuprammonium cellulose together with a silicon compound having the structure RBiHzDI-I in which R represents an alkyl radical, said compound being stable vin said solution,

6. As a new article of manufacture, regenerated cellulose containing a finely dispersed substance of the group consisting of aliphatic silicon compounds having the structure R.SiI-Ia in which R.

represents an alkyl radical, aliphatic silicon com- I RUDOLPH B. BLEY. 

